The preparation technique of methyl anthranilate comprises the following actions:
( 1) 25% ammoniacal liquor of 937kg10 ℃ is put into amidation reactor, 1000kg phthalic anhydride is dropped in the amidation reactor, as well as ammoniacal alcohol as well as phthalic anhydride respond in the atmosphere listed below 30 ℃ to generate o-formamide benzoic acid ammonium, react Time 2.5 h. The 25% ammoniacal liquor that actually takes part in the amidation response is 892.3 kg, and 937kg of 25% ammoniacal liquor is included for the amidation response to be extra total.
( 2) After the amidation response, took into the sodium hydroxide solution of 879kg30% in the amidation activator, o-formamide benzoic acid ammonium and salt hydroxide generation variation response produce sodium o-formamide benzoate, then the amidation reactor The temperature inside rises to 50 ° C, as well as the ammonia molecules in the mixed remedy are vaporized, and the vaporized ammonia gas is led by the induced draft follower to the two-stage collection water absorption tower for water absorption to obtain ammonia water, and also the ammonia water is sent to the ammonia water storage tank, and then to the ammonia water tank Add fluid ammonia inside to make 25% ammonia water for reuse.
( 3) place the remedy in the amidation reactor right into the esterification reactor, put into the methanol option of 1561kg75% as well as the salt hypochlorite option of 3451kg14% in the reactor, maintain the temperature level in the esterification activator to be 10 DEG C, react A paste-like methyl anthranilate was created, as well as the response time was 3 hrs. After the response, the temperature level in the esterification reactor was raised to 50 ° C. Add 1000kg hot water in the esterification reactor after the liquifying of pasty methyl anthranilate.
( 4) Send the solution in the esterification reaction kettle into the methyl ester settling container as well as let it mean separation. The option in the top layer is pumped into the methanol recovery procedure, as well as the remedy in the lower layer is filtered by a jet vacuum pump to acquire the filtrate. Stand still as well as different, pump the remedy in the upper layer right into the methanol healing process, put the filtrate in the reduced layer into the purification pot, and carry out purification in an environment with a stress of 2.00 Kpa and also a temperature level of 135.5 ° C to obtain a finished item.
The remedy sent to the methanol healing process is pumped right into the methanol rectification tower. Making use of the different boiling points of the elements in the service, the methanol in the service is vaporized first, as well as the methanol vapor is condensed to acquire a methanol remedy. The remaining remedy is cooled as well as crystallized. Send it to the centrifuge, and also after centrifugation, it can be offered as commercial salt.
A kind of one-step approach creates the manufacturing method of methyl anthranilate, particularly makes up the complying with steps:
( 1) Add 18.2 g of N-chlorophthalimide, 6.4 g of methanol and 40g of water into a three-necked flask, after that reduced the temperature to listed below 0 ° C, as well as stir to make a slurry.
( 2) Add 16.2 g of 30% sodium hydroxide aqueous remedy dropwise, after dropping, keep the temperature listed below 0 ° C and mix for 20 minutes;
( 3) After raising the temperature to 50-80 ° C. for one hr, the temperature level was normally decreased, and also the layers were divided for ten hrs, as well as the item 13.8 g of methyl anthranilate was acquired in the lower layer. The item purity is 99.8%, and also the return is 91.4%.
1. First include ammonia water with a proportion of 0.115 to 0.135 components (relative to phthalic anhydride) in the amidation response kettle, start stirring, add 1 part of phthalic anhydride within one min, and include a proportion of 0.27 parts (relative to phthalic anhydride) Part to 0.90 parts of liquid caustic soda, to make it undergo amidation reaction, and also always make certain that the pH value is more than 7 during the manufacturing of amidation fluid. When the pH worth gets to 8.5, stop adding fluid caustic soda, after completely stirring, the amidated liquid that creates is discharged ammonia;
2. Pump the amidation remedy after wearing down ammonia right into the esterification response pot, include 0.216 parts to 1 part of methanol symmetrical (about phthalic anhydride), cool to listed below -15 ° C, and after that include 4 components below zero ~ 5 parts of sodium hypochlorite option with a mass concentration of 11% undergo Hofmann destruction reaction to produce methyl anthranilate solution;
3. Put the produced methyl anthranilate remedy right into the filter through the pump, filter, as well as the filtered option enters the methyl ester formation storage tank, begin stirring, cool down to listed below 24 ° C, and make the methyl anthranilate
remedy The crystallization of methyl ester is separated out, acquires solid methyl ester through purification;
4. Pump the filtered filtrate right into the alkali removal pot, cool down to listed below 0 ° C, and also precipitate water antacids (sodium carbonate decahydrate);.
5. The filtrate after filtering the water alkali (sodium carbonate decahydrate) is pumped into the purification tower, evaporated, and the obtained gas phase recuperates methanol;.
6. The purification raffinate at the bottom of the distillation tower redeems anthranilic acid;.
7. The drainage consisting of less than 3% salt after recovering anthranilic acid is treated for waste water.
